ANALYTICAL INSTRUMENTATION

INTRODUCTION
Based on the physical and chemical properties of matter, the analysers could be broadly classified into 4 catagories that the matter is having some interaction with energy. These energy states which may be characteristics of any chemical composition and this external energy source may be in any of the basic groups.

GROUPS
Electromagnetic Radiation - Group - I

Chemical affinity or Reactivity - Group II Electric or Magnetic fields - Group - III

Thermal or Mechanical energy- Group - IV

Group - I
Measurement of the quantity and quality of electromagnetic radiation emitted, reflected, transmitted or diffracted by the sample, by which the molecular composition of solid, liquid, or gas may be analysed.

Group - II
Determination of chemical composition by measurement of the reaction product with other chemicals in terms of amount of sample or reactant consumed, product formed or thermal energy liberated or determination of equilibrium attained is the basis for most of the classical methods of qualitative and quantitative chemical analysis.

Group II (Cont.)
Several instrumental methods have been applied to this technique and it involves two steps. a) Promotion of a chemical reaction. b) Measurement of a reaction product as a means for determining the presence and quantity of a particular constituent in the sample.

GROUP -III
Measurement of the current, voltage, or flux change produced in the energised electric and magnetic circuits containing the sample. The production of net electric charges on atoms or molecules by bombardment with ionizing particles or radiation or by electrolysis or dissociation in solution or the induction of dipoles by strong fields establishes measurable relationships between these ion.

GROUP - IV
Measurements of the results of applying thermal or mechanical energy to a system in terms of energy transmission, work done, or changes in physical state.

Thermodynamic relationship involving the physical state and thermal energy content of any substance permits analysis and identification of mixture of solids, liquids and gases based upon the freezing and boiling points and upon the quantitative measurement of physically separated fractions. Useful information can often be derived from thermal conductivity and viscosity measurements.

ANALYZER TYPES
pH Analyzer Oxygen Analyzer Infra red Analyzers Thermal Conductivity Analyzers Electrode-less conductivity Analysers Gas chromatograph. Liquid chromatograph. Gas detectors. Hydro Carbon leakage detectors.

pH Analyzer
The term pH is a convention used to indicate the acidity or alkalinity of a solution. It is obtained by determining the logarithm (base 10) of the reciprocal of hydrogen ion concentration expressed is grams/liter.

Electrodes in pH Analyzer
Glass electrode. Reference electrode. Sensing element for temp. Compensator.

Glass Electrode
The primary function of the Glass electrode is to develop a potential proportional to the hydrogen ion concentration. This potential is used to represent the pH value in the pH meter

Reference Electrode
The reference electrode is designed to produce a constant potential regardless of the solution in which it is immersed. For further details. Ref. API-RP-550-part-II. manual for reference

Oxygen Analyzer
It works on paramagnetic principle admits gases in vicinity of a hot wire inside a non uniform magnetic field, then the gas is heated reducing its magnetic susceptibility causing it to be displaced by the incoming cooler gas experiencing a strong magnetic force thus a form of wind is created, thus there was a flow of oxygen molecules drawing other molecules with them and causing cooling of one coil and heating of the other. The change in resistance of the coils was monitored and calibrated in percentage of oxygen.

Oxygen Analyzer
Chemical method This method is suitable for the determination of oxygen content in non combustible gases or saturated hydrocarbons. The method is based upon the measurement of the change in temperature due to the total catalytic combustion of the oxygen in the sample with hydrogen.

Oxygen Analyzer - Thermal Conductivity

The sample gas at room temperatures mixed with a constant stream of hydrogen. The mixer is admitted to one chamber of a dual thermal conductivity detector, after which the oxygen in the sample is reacted with the hydrogen in a suitable oven to form water. The remaining mixer after the removal of its water content is admitted to the second chamber of the detector. The unbalance in the conductivity bridge is directly proportional to the oxygen concentration.

INFRA RED ANALYZERS

There are two major groups of infra red Analysers depending upon the means of wavelength selection. The dispersive type. The non dispersive type.

DISPERSIVE TYPE INFRA RED ANALYSER

The instrument uses a grating Monochromator with two entrance slits to yield two wavelengths, one monochromator at the measuring wavelength of the desired component in the liquid sample and one monochromator at an appropriate reference wavelength. The detector is a radiation thermocouple as used in laboratory instruments.

NON DISPERSIVE TYPE INFRA RED ANALYSER

The sample cell is highly polished tube that conducts the radiant energy through it by multiple reflection. The gaseous sample from the process flows continuously through this cell. The reference cell is similar but generally is used only to transmit the radiant signal and is simply filled with inert gas. The radiant energy then passes into the pneumatic microphone detector. The detector is a sealed chamber with the very thin flexible diaphragm separating the two halves exposed to each beam. Thus changing the relative pressure in the two chambers. The pressure change deflects the flexible diaphragm which forms a variable capacitor plate in an electric circuit.

Band pass optical filter Analyzer

This instrument can be built to operate in the entire infra-red region. The variable wavelength wedge type interference filter analyzer simplifies the monochromator portion of a dispersive-type analyzer. The filter replaces the entire monochromator in its function of isolating the operating wavelength.

THERMAL CONDUCTIVITY ANALYZERS

A wheatstone bridge is the form of network employed to measure the resistance change of the sensing element. The current used to energise the bridge also serve for heating the wire. It is common practice to use two cells in adjacent arms, one of the cells containing the reference gas and other containing the gas to be analyzed. The bridge then responds to the difference in temperature rise (ie resistance) of the two sensing elements and thus is dependent upon the difference in thermal conductivities of the gases in the two cells.

ELECTRODELESS CONDUCTIVITY ANALYSER

Electrodeless type conductivity cells are ideally suited where the use of conventional electrode type cells is difficult, impractical, or even impossible due to the nature of the solution being measured. Solutions which are oily, corrosive, abrasive, or which contain entangling fibres are natural applications for the electrodeless cell. Maintenance problems associated with such solutions are reduced to a minimum allowing years of uninterrupted service.

GAS CHROMATOGRAPH
The gas chromatograph is a device which is used for making qualitative and quantitative analysers of selected stream components and for promptly supplying information equivalent to that obtained from a refinery control laboratory. The purpose of the gas chromatograph is to determine the quantities of individual components or combinations of components to the extent necessary for intelligent operation of a process. It can be used for the following.

Uses
Single Key Component Analysis. Multi Component Analysis (Single Stream) Complete Analysis (Single Stream) Multistream Analysis (either partial or complete)

LIQUID CHROMATOGRAPH
The operating conditions are very stringent and the sample valves for liquids should be precise and the volume of sample allowed must be between 0.2 to 20 Micro liters, and must not vary more than 1 percent for successive samples.

 Partition columns are used in gas - liquid chromatography for separating complex hydrocarbon samples. The separating medium (the column packing) is a granular solid impregnated with a liquid substrate that is essentially non-volatile under the conditions of use. The packing appears to be dry but in reality exposes a large liquid surface to the vaporised sample component as they are bourne through the column by the carrier gas. The sample components are partitioned between the gas and liquid phases. Those components least soluble in the liquid pass rapidly through the columns and emerge early. Those components most soluble in the liquid are retarded and emerged later. The most volatile components generally emerge earliest.